CN102942379B - Preparation method of Y4Si3O12 crystal whisker toughening Y4Si3O12 composite coatings - Google Patents

Preparation method of Y4Si3O12 crystal whisker toughening Y4Si3O12 composite coatings Download PDF

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CN102942379B
CN102942379B CN 201210458353 CN201210458353A CN102942379B CN 102942379 B CN102942379 B CN 102942379B CN 201210458353 CN201210458353 CN 201210458353 CN 201210458353 A CN201210458353 A CN 201210458353A CN 102942379 B CN102942379 B CN 102942379B
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whisker
y4si3o12
powder
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CN102942379A (en
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黄剑锋
杨柳青
曹丽云
王雅琴
费杰
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Yan Sanyuan
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a preparation method of Y4Si3O12 crystal whisker toughening Y4Si3O12 composite coatings. According to the preparation method, firstly, an embedding method is adopted for preparing a SiC (silicon carbide) porous inner coating on the base body surface of a C/C (carbon/carbon) composite material, then, Y4Si3O12 crystal whiskers are prepared, in addition, composite surfactants are adopted for carrying out surface modification on the Y4Si3O12 crystal whiskers, and mixed liquid is obtained; and the C/C composite material with the SiC porous inner coating prepared on the surface and the mixed liquid are adopted for carrying out ultrasonic electrophoresis selective assembly deposition, a Y4Si3O12 crystal whisker pinning layer is obtained, and finally, the Y4Si3O12 crystal whisker toughening Y4Si3O12 composite coatings are prepared by a hydrothermal electrophoretic deposition method. The Y4Si3O12 crystal whisker toughening Y4Si3O12 composite coatings prepared by the preparation method are uniform and compact, no microscopic cracks exist, and the bonding force between the base body and the inner coating as well as between the inner coating and the outer coating is obviously improved. The prepared Y4Si3O12 crystal whisker toughening Y4Si3O12 composite coatings can realize the effective protection on the C/C composite material for 350 hours in static air at 1700 DEG C, and the oxidation weightless rate is smaller than 0.8 percent.

Description

A kind of Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the preparation method of compound coating
Technical field
The invention belongs to the C/C technical field of composite materials, relate to a kind of preparation method of C/C matrix material high-temperature oxidation resistant coating, be specifically related to a kind of Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the preparation method of compound coating.
Background technology
Carbon/carbon (C/C) matrix material has the excellent properties such as thermal expansivity is low, density is low, high temperature resistant, anti-ablation, high strength, high-modulus, particularly 2200 ℃ of inert atmosphere with interior condition under its strength and modulus excellent properties of raising and increase with temperature, it is had broad application prospects at aerospace field.Yet the C/C matrix material will be oxidized at the aerobic environment that surpasses 450 ℃, the oxidation quality loss causes its strength degradation, has limited its practical application.Therefore, solving C/C matrix material high-temp antioxidizing problem is the key that takes full advantage of its performance.
Improve the C/C compound material antioxygenic property and mainly contain two kinds of approach: a kind of is the matrix modification technology; A kind of is the top coat technology.Research shows, the matrix modification technology is only applicable to the oxidation protection of low-temperature zone to the C/C material.Coating technology can solve the high temperature oxidation problem of C/C material.
The more C/C matrix material high-temperature oxidation resistant coating of research has SiC[Y.L.Zhang at present, H.J.Li, Q.G.Fu.A C/SiC gradient oxidation protective coating for carbon/carboncomposites.Surf.Coaf.Techol., 2006,201:3491-3495.], CrSi 2[Fu Qian-Gang, LiHe-Jun, Shi Xiao-Hong.A SiC whisker-toughened SiC-CrSi 2oxidation protectivecoating for carbon/carbon composites, April.Surf.Sci., 2007,253:3757-3760.], Si-Mo[Zhi-Qiao Yan, Xiang Xiong, Peng Xiao, Feng Chen, Hong-Bo Zhang, Bai-Yun Huang.A multilayer coating of dense SiC alternated with porous Si-Mofor the oxidation protection of carbon/carbon composites, Carbon, 2008,46 (1): 149-153.], Si-MoSi 2[Yu-Lei Zhang, He-Jun Li, Xi-Yuan Yao.Oxidation protectionof C/SiC coated carbon/carbon composites with Si-Mo coating at hightemperature, Corros.Sci., 2011,53:2075-2079.], Mo-Si-N[Z.H.Lai, J.C.Zhu, J.H.Jeon.Phase constitutions of Mo-Si-N anti-oxidation multi-layer coatings onC/C composites by fused slurry.Mater.Sci.Eng.A, 2009,499:267-270.] and Si-Mo-SiO 2[Z.Q.Yan, X.Xiong, P.Xiao, et al.Si-Mo-SiO 2oxidation protectivecoatings prepared by slurry painting for C/C-SiC composites.Surf.Coaf.Techol., 2008,202:4734-4740.] etc., Huang Jianfeng etc. have also studied take other compound coating that SiC is transition layer, as SiC-B 4c/SiC/SiO 2[Jun Li, Ruiying Luo, Chen Lin.Oxidation resistance of agradient self-healing coating for cabon/carbon composites, Carbon, 2007,45:2471-2478], SiC/Y 2siO 5[Argirusis C hr., Damjanovic T., Borchardt G..Yttriumsilicate coating system for oxidation protection of C/C-Si-SiC composites:Electrophoretic deposition and oxygen self-diffusion measurements, Journal of theEuropean Ceramic Society, 2007,27 (2-3): 1303-1306.] and SiC/MoSi 2-CrSi 2-Si[Li-He-Jun, Feng Tao, Fu Qian-Gang.Oxidation and erosionresistance of MoSi 2-CrSi 2-Si/SiC coated C/C composites in static and aerodynamicoxidation environment, Carbon, 2012,48:1636-1642.] etc.Yet above-mentioned coating does not also reach 1600 ~ 2500 ℃ of application request under the Fast ion flow Scouring Condition, the high-temperature oxidation resistant ceramic coating of carbon/carbon compound material high-speed fuel gas wash away under environment easily come off and the oxidation protection time short,
Summary of the invention
The object of the present invention is to provide a kind of Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the preparation method of compound coating, prepared compound coating is fine and close, force of cohesion is good and high-temperature oxidation resistance is excellent, can extend in combustion gas and wash away under dynamic environment the protection against oxidation time to the C/C matrix material.
For achieving the above object, the technical solution used in the present invention is:
Step 1: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, get commercially available analytically pure Si powder, C powder and Cr 2o 3powder, press the Si powder: C powder: Cr 2o 3powder=(4 ~ 5): (5 ~ 6): the mass ratio preparation embedding powder of (0.5 ~ 1.0), then pretreated carbon/carbon compound material is put into to plumbago crucible, and it is imbedded in the embedding powder;
2) secondly, plumbago crucible is put into to vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 10 ~ 30 ℃/min, by furnace temperature from room temperature rises to 1500 ~ 1700 ℃, with the stove naturally cooling, will complete the carbon/carbon compound material ultrasonic cleaning 0.5 ~ 1h of embedding with dehydrated alcohol after insulation 1 ~ 3h, ultrasonic power is 300 ~ 500W;
3) last, in the electric drying oven with forced convection of 50 ~ 80 ℃, drying obtains with the internally coated carbon/carbon compound material of SiC porous;
Step 2: adopt complexed surfactant to Y 4si 3o 12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.5 ~ 0.8mol/L, by Y 4si 3o 12whisker (is shown in patent " a kind of Y 4si 3o 12the preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in solution, ultrasonic radiation 30 ~ 50min, ultrasonic power is 400 ~ 600W, then filters and isolate Y 4si 3o 12whisker;
2) by separating obtained Y 4si 3o 12whisker and Virahol are pressed Y 4si 3o 12whisker: Virahol=(10 ~ 20g): the ratio of (150 ~ 300ml) is mixed with suspension, then in suspension, by (0.6 ~ 0.8) g/mL, adds iodine, stirs and obtains mixed solution;
Step 3: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 4si 3o 12the whisker pinning layer:
1) mixed solution step 2 made is placed in the ultrasonic electric deposition apparatus, prepared by the step 1 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, it is 300 ~ 500W that ultrasonic power is controlled, and temperature is 40 ~ 60 ℃, and deposition voltage is 20 ~ 40V, deposition current is 0.05 ~ 0.1A, and depositing time is 3 ~ 10min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 3 ~ 5 times, 80 ~ 120 ℃ of dryings, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the whisker pinning layer;
Step 4: adopt the standby Y of water heat electrophoresis deposition legal system 4si 3o 12crystal whisker toughened Y 4si 3o 12compound coating:
1) get 10 ~ 30g Y 4si 3o 12powder is suspended in the Virahol of 100 ~ 300ml, and magnetic agitation 10 ~ 30h adds the iodine of 0.04 ~ 0.12g subsequently, and magnetic agitation 10 ~ 30h, be prepared into suspension;
2) with step 3, make with Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in the water heat electrophoresis deposition reactor, and controlling packing ratio is 40 ~ 60%, insulation after being heated to 140 ~ 180 ℃, adjusting deposition voltage is that 160 ~ 220V carries out water heat electrophoresis deposition, stops energising after depositing 20 ~ 30min, after sample is cooling, takes out, the baking oven that is placed in 60 ~ 80 ℃ is dry, obtains with Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the C/C matrix material sample of compound coating.
Described Si powder, C powder and Cr 2o 3the granularity of powder is 20 ~ 30 μ m.
The described C/C matrix material pre-treatment following steps of guaranteeing replacement:
1) get the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 10 * 10 * 10 ~ 20 * 20 * 20mm 3cubes, and, to the surface treatment of its chamfering of being polished, chamfering is 30 ~ 50 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 10 ~ 30min at every turn, and ultrasonic power is 80 ~ 120W, finally dry in the electric drying oven with forced convection of 50 ~ 80 ℃.
Described Y 4si 3o 12the granularity of powder is 20 ~ 30 μ m.
Due to Y 4si 3o 12fusing point be 1950 ℃, its thermal expansivity is 4.3 * 10 -6k -1, with the thermal expansivity (4.5 * 10 of SiC -6k -1) very approaching, Y 4si 3o 12can effectively prevent coating high-temp cracking and the problem come off as the external coating (EC) of being combined with the SiC undercoat, simultaneously with Y 4si 3o 12whisker is as the toughening material of compound coating, utilize between same substance and good physical chemistry consistency, effectively improve the bonding force between compound coating and carbon/carbon compound material, inside and outside coating, when improving the antiscour shear stress, also can greatly improve antioxidant property.
Beneficial effect:
1. the Y that the present invention makes 4si 3o 12crystal whisker toughened Y 4si 3o 12compound coating is even, densification, and without micro-flaw, the bonding force between matrix and undercoat and inside and outside coating obviously improves.
2. the Y that the present invention makes 4si 3o 12crystal whisker toughened Y 4si 3o 12compound coating can carry out effective protection of 350h in the still air of 1700 ℃ to the C/C matrix material, oxidative mass loss is less than 0.8%.
The accompanying drawing explanation
The Y that Fig. 1 is embodiment 1 preparation 4si 3o 12crystal whisker toughened Y 4si 3o 12the SEM photo of compound coating section.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail.
Embodiment 1:
The pre-treatment of step 1:C/C matrix material:
1) get the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 15 * 15 * 15mm 3cubes, and, to the surface treatment of its chamfering of being polished, chamfering is 30 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 20min at every turn, and ultrasonic power is 80W, last dry in the electric drying oven with forced convection of 50 ℃.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, get Si powder, C powder and the Cr that commercially available analytically pure granularity is 20 ~ 30 μ m 2o 3powder, press the Si powder: C powder: Cr 2o 3the mass ratio preparation embedding powder of powder=4:5.5:0.5, then put into plumbago crucible by pretreated carbon/carbon compound material, and it imbedded in the embedding powder;
2) secondly, plumbago crucible is put into to vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 10 ℃/min, by furnace temperature from room temperature rises to 1500 ℃, with the stove naturally cooling, will complete the carbon/carbon compound material ultrasonic cleaning 0.5h of embedding with dehydrated alcohol after insulation 3h, ultrasonic power is 300W;
3) last, in the electric drying oven with forced convection of 50 ℃, drying obtains with the internally coated carbon/carbon compound material of SiC porous;
Step 3: adopt complexed surfactant to Y 4si 3o 12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.5mol/L, by Y 4si 3o 12whisker (is shown in patent " a kind of Y 4si 3o 12the preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in solution, ultrasonic radiation 30min, ultrasonic power is 600W, then filters and isolate Y 4si 3o 12whisker;
2) by separating obtained Y 4si 3o 12whisker and Virahol are pressed Y 4si 3o 12the ratio of whisker: Virahol=10g:230ml is mixed with suspension, then in suspension, by 0.6g/mL, adds iodine, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 4si 3o 12the whisker pinning layer:
1) mixed solution step 3 made is placed in the ultrasonic electric deposition apparatus, prepared by the step 2 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled as 300W, and temperature is 40 ℃, and deposition voltage is 30V, deposition current is 0.05A, and depositing time is 3min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 3 ~ 5 times, 80 ℃ of dryings, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the whisker pinning layer;
Step 5: adopt the standby Y of water heat electrophoresis deposition legal system 4si 3o 12crystal whisker toughened Y 4si 3o 12compound coating:
1) get the Y that the 10g granularity is 20 ~ 30 μ m 4si 3o 12powder is suspended in the Virahol of 200ml, and magnetic agitation 10h adds the iodine of 0.04g subsequently, and magnetic agitation 10h, be prepared into suspension;
2) with step 4, make with Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in the water heat electrophoresis deposition reactor, and controlling packing ratio is 40%, insulation after being heated to 140 ℃, adjusting deposition voltage is that 160V carries out water heat electrophoresis deposition, after deposition 30min, stops energising, after sample is cooling, takes out, the baking oven that is placed in 60 ℃ is dry, obtains with Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the C/C matrix material sample of compound coating.
Y as seen from Figure 1 4si 3o 12whisker is at porous SiC undercoat and Y 4si 3o 12directed interting between external coating (EC), the compound coating even compact, do not have crackle.
Embodiment 2:
The pre-treatment of step 1:C/C matrix material:
1) get the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 10 * 10 * 10mm 3cubes, and, to the surface treatment of its chamfering of being polished, chamfering is 40 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 30min at every turn, and ultrasonic power is 100W, last dry in the electric drying oven with forced convection of 65 ℃.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, get Si powder, C powder and the Cr that commercially available analytically pure granularity is 20 ~ 30 μ m 2o 3powder, press the Si powder: C powder: Cr 2o 3the mass ratio preparation embedding powder of powder=5:5:0.8, then put into plumbago crucible by pretreated carbon/carbon compound material, and it imbedded in the embedding powder;
2) secondly, plumbago crucible is put into to vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 20 ℃/min, by furnace temperature from room temperature rises to 1600 ℃, with the stove naturally cooling, will complete the carbon/carbon compound material ultrasonic cleaning 1h of embedding with dehydrated alcohol after insulation 2h, ultrasonic power is 400W;
3) last, in the electric drying oven with forced convection of 80 ℃, drying obtains with the internally coated carbon/carbon compound material of SiC porous;
Step 3: adopt complexed surfactant to Y 4si 3o 12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.6mol/L, by Y 4si 3o 12whisker (is shown in patent " a kind of Y 4si 3o 12the preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in solution, ultrasonic radiation 40min, ultrasonic power is 500W, then filters and isolate Y 4si 3o 12whisker;
2) by separating obtained Y 4si 3o 12whisker and Virahol are pressed Y 4si 3o 12the ratio of whisker: Virahol=15g:150ml is mixed with suspension, then in suspension, by 0.7g/mL, adds iodine, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 4si 3o 12the whisker pinning layer:
1) mixed solution step 3 made is placed in the ultrasonic electric deposition apparatus, prepared by the step 2 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled as 400W, and temperature is 50 ℃, and deposition voltage is 20V, deposition current is 0.08A, and depositing time is 6min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 3 ~ 5 times, 100 ℃ of dryings, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the whisker pinning layer;
Step 5: adopt the standby Y of water heat electrophoresis deposition legal system 4si 3o 12crystal whisker toughened Y 4si 3o 12compound coating:
1) get the Y that the 20g granularity is 20 ~ 30 μ m 4si 3o 12powder is suspended in the Virahol of 100ml, and magnetic agitation 20h adds the iodine of 0.08g subsequently, and magnetic agitation 20h, be prepared into suspension;
2) with step 4, make with Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in the water heat electrophoresis deposition reactor, and controlling packing ratio is 50%, insulation after being heated to 160 ℃, adjusting deposition voltage is that 200V carries out water heat electrophoresis deposition, after deposition 26min, stops energising, after sample is cooling, takes out, the baking oven that is placed in 70 ℃ is dry, obtains with Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the C/C matrix material sample of compound coating.
Embodiment 3:
The pre-treatment of step 1:C/C matrix material:
1) get the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 20 * 20 * 20mm 3cubes, and, to the surface treatment of its chamfering of being polished, chamfering is 50 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 10min at every turn, and ultrasonic power is 120W, last dry in the electric drying oven with forced convection of 80 ℃.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, get Si powder, C powder and the Cr that commercially available analytically pure granularity is 20 ~ 30 μ m 2o 3powder, press the Si powder: C powder: Cr 2o 3the mass ratio preparation embedding powder of powder=4.5:6:1.0, then put into plumbago crucible by pretreated carbon/carbon compound material, and it imbedded in the embedding powder;
2) secondly, plumbago crucible is put into to vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 30 ℃/min, by furnace temperature from room temperature rises to 1700 ℃, with the stove naturally cooling, will complete the carbon/carbon compound material ultrasonic cleaning 1h of embedding with dehydrated alcohol after insulation 1h, ultrasonic power is 500W;
3) last, in the electric drying oven with forced convection of 65 ℃, drying obtains with the internally coated carbon/carbon compound material of SiC porous;
Step 3: adopt complexed surfactant to Y 4si 3o 12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.8mol/L, by Y 4si 3o 12whisker (is shown in patent " a kind of Y 4si 3o 12the preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in solution, ultrasonic radiation 50min, ultrasonic power is 400W, then filters and isolate Y 4si 3o 12whisker;
2) by separating obtained Y 4si 3o 12whisker and Virahol are pressed Y 4si 3o 12the ratio of whisker: Virahol=20g:300ml is mixed with suspension, then in suspension, by 0.8g/mL, adds iodine, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 4si 3o 12the whisker pinning layer:
1) mixed solution step 3 made is placed in the ultrasonic electric deposition apparatus, prepared by the step 2 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled as 500W, and temperature is 60 ℃, and deposition voltage is 40V, deposition current is 0.1A, and depositing time is 10min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 3 ~ 5 times, 120 ℃ of dryings, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the whisker pinning layer;
Step 5: adopt the standby Y of water heat electrophoresis deposition legal system 4si 3o 12crystal whisker toughened Y 4si 3o 12compound coating:
1) get the Y that the 30g granularity is 20 ~ 30 μ m 4si 3o 12powder is suspended in the Virahol of 300ml, and magnetic agitation 30h adds the iodine of 0.12g subsequently, and magnetic agitation 30h, be prepared into suspension;
2) with step 4, make with Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in the water heat electrophoresis deposition reactor, and controlling packing ratio is 60%, insulation after being heated to 180 ℃, adjusting deposition voltage is that 220V carries out water heat electrophoresis deposition, after deposition 20min, stops energising, after sample is cooling, takes out, the baking oven that is placed in 80 ℃ is dry, obtains with Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the C/C matrix material sample of compound coating.

Claims (4)

1. a Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the preparation method of compound coating is characterized in that:
Step 1: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, get commercially available analytically pure Si powder, C powder and Cr 2o 3powder, press the Si powder: C powder: Cr 2o 3powder=(4～5): (5～6): the mass ratio preparation embedding powder of (0.5～1.0), then pretreated C/C matrix material is put into to plumbago crucible, and it is imbedded in the embedding powder;
2) secondly, plumbago crucible is put into to vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 10～30 ℃/min, by furnace temperature from room temperature rises to 1500～1700 ℃, after insulation 1～3h, with the stove naturally cooling, the C/C compound material ultrasound that will complete embedding with dehydrated alcohol cleans 0.5～1h, and ultrasonic power is 300～500W;
3) last, in the electric drying oven with forced convection of 50～80 ℃, drying obtains with the internally coated C/C matrix material of SiC porous;
Step 2: adopt complexed surfactant to Y 4si 3o 12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.5～0.8mol/L, by Y 4si 3o 12whisker is immersed in solution, ultrasonic radiation 30～50min, and ultrasonic power is 400～600W, then filters and isolate Y 4si 3o 12whisker;
2) by separating obtained Y 4si 3o 12whisker and Virahol are pressed Y 4si 3o 12whisker: Virahol=(10～20g): the ratio of (150～300mL) is mixed with suspension, then in suspension, by (0.6～0.8) g/mL, adds iodine, stirs and obtains mixed solution;
Step 3: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 4si 3o 12the whisker pinning layer:
1) mixed solution step 2 made is placed in the ultrasonic electric deposition apparatus, prepared by the step 1 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, it is 300～500W that ultrasonic power is controlled, and temperature is 40～60 ℃, and deposition voltage is 20～40V, deposition current is 0.05～0.1A, and depositing time is 3～10min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 3～5 times, 80～120 ℃ of dryings, with porous SiC, on internally coated C/C matrix material, obtaining Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the whisker pinning layer;
Step 4: adopt the standby Y of water heat electrophoresis deposition legal system 4si 3o 12crystal whisker toughened Y 4si 3o 12compound coating:
1) get 10～30g Y 4si 3o 12powder is suspended in the Virahol of 100～300mL, and magnetic agitation 10～30h adds the iodine of 0.04～0.12g subsequently, and magnetic agitation 10～30h, be prepared into suspension;
2) with step 3, make with Y 4si 3o 12whisker embeds the Y of SiC hole 4si 3o 12the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in the water heat electrophoresis deposition reactor, and controlling packing ratio is 40～60%, insulation after being heated to 140～180 ℃, adjusting deposition voltage is that 160～220V carries out water heat electrophoresis deposition, stops energising after depositing 20～30min, after sample is cooling, takes out, the baking oven that is placed in 60～80 ℃ is dry, obtains with Y 4si 3o 12crystal whisker toughened Y 4si 3o 12the C/C matrix material sample of compound coating.
2. Y according to claim 1 4si 3o 12crystal whisker toughened Y 4si 3o 12the preparation method of compound coating is characterized in that: described Si powder, C powder and Cr 2o 3the granularity of powder is 20～30 μ m.
3. Y according to claim 1 4si 3o 12crystal whisker toughened Y 4si 3o 12the preparation method of compound coating is characterized in that: the pre-treatment of described C/C matrix material comprises the following steps:
1) get the 2D-C/C matrix material that the aircraft brake sheet is used, be processed into 10 * 10 * 10～20 * 20 * 20mm 3cubes, and, to the surface treatment of its chamfering of being polished, chamfering is 30～50 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3～5 times, clean ultrasonic time is 10～30min at every turn, and ultrasonic power is 80～120W, last dry in the electric drying oven with forced convection of 50～80 ℃.
4. Y according to claim 1 4si 3o 12crystal whisker toughened Y 4si 3o 12the preparation method of compound coating is characterized in that: described Y 4si 3o 12the granularity of powder is 20～30 μ m.
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